XRF Report Nr. XRF-70, Rev. 2 SPECTRO XHH03 Summary Excitation of the fluorescence radiation in the sample by an X-ray tube has been optimized so that extremely short measuring times with a high sample throughput are possible. Specially developed detector technology, based on SDD, enables high signal throughput at high resolution; allowing for a unique analytical flexibility and a considerably accelerated signal processing. With the SPECTRO it is possible to conduct laboratory-like analyses in a single measuring cycle that lasts only 2 seconds, except for the light elements Mg, Al,, P and S they require a longer measurement time. Only 10 additional seconds are necessary for the sorting of various aluminum and magnesium alloys. During this process even the light elements Al, Mg,, P and S are measured in air without complicated additional techniques like helium flushing or vacuum, simplifying operation decidedly. The analysis screen supplies the operator with all of the necessary information at a single glance and can display the measurement result in different views - also during measurement. The analytical results are stored and can be displayed later, printed and, after transfer to an external computer, processed with the Result Manager software. of Solid Metal Samples SPECTRO Analytical Instruments GmbH, Kleve, Germany 1. Introduction SPECTRO products are viewed around the world as standards for onsite metal analysis. No other company possesses comparable knowhow and similarly comprehensive experience in this area. As one of the leading international manufacturers of XRF instruments, laboratory analyses with extremely powerful X-ray fluorescence spectrometers is also an area in which SPECTRO excels. With the new SPECTRO, SPECTRO introduces a compact energy dispersive X-ray fluorescence spectrometer for the continuous, fatigue-free handheld analysis and sorting of metals. It makes use of innovative efficient components for excitation and detection. Together with other top quality modules, they are the basis for the unique precision, speed and safety of this system; combining the experience with onsite metal analysis and the demands for laboratory quality measurement results. Page 1/10
2. Instrumentation To test an alloy group, SPECTRO calibration modules are preinstalled on the SPECTRO. There are three different modules available. For example, the testing of stainless steels requires the Standard calibration module. The measurement of magnesium or aluminum based alloys requires the calibration module Light Elements and the measurement of precious metal alloys, the module Precious Metals. A single measuring cycle lasts only 2 seconds for the modules Standard and Precious Metals. Only 10 seconds in addition are necessary for both the sorting of various aluminum and magnesium alloys and the analysis of different alloys including Al,, P and S with the module Light Elements. 3. Technical Data Detector High resolution silicon drift detector (SDD) Excitation X-ray tube with Rh anode up to 50 kv tube voltage Operation A sample name can be entered and then the start button can be released after the first result is displayed on the screen, or continue to press until the preset measurement time is elapsed. Spectrometer Control epc including Windows mobile operating system Automatic drift correction SD card slot Bluetooth, Wireless LAN, USB Dimensions and Weight Height: 270 mm (10,7 ) Width: 93 mm (3.7 ) Depth: 230 mm (9.1 ) Weight Instrument: 1.64 kg (3.62 lbs) including Battery pack Power/ Electrical Connection Battery operation with Li-Polymer batteries, rechargeable (4 h typical duty cycle) 100-240 V, +/- 10 %, 50 / 60 Hz (AC adapter/ charger) 11 W during analysis 6 W Standby mode 3 W Offline mode Options Additional battery pack Barcode reader (Bluetooth) Printer (Bluetooth) Wireless data transfer kit Small parts adapter Video camera Internal GPS receiver Docking station Accessories (Included) Transport case Instrument/battery holster Two battery packs Charger/ AC adapter USB cable Consumables Software Eval-Server for data treatment and fundamental parameter analysis ICAL (Intelligent Calibration Logic) Result Manager: post-processing of stored measurement values and protocols Mode Automatic fingerprint analysis Automatic average calculation Calculation standard deviation and relative standard deviation Page 2/10
Grade ID Mode Grade identification based on stored library of grade specifications Grade verification, based on selected grade specification Optional display of analysis and/or grade identification Grade library easily edited and expanded Sorting Mode Fast pass/fail assessment based on a reference sample Symmetrical and asymmetrical tolerances allowed Three modes of operation to suit different sorting tasks Log reports Documentation Basic operator manual Back up on USB-flash drive 4. Sample Preparation To enhance accuracy samples can be prepared with grinding paper (approx. 60 or 80 grit aluminum or zirconium oxide) or a milling machine can be used. For grade identification in most cases no sample preparation is necessary. On most finished parts sample preparation is not necessary. 5. Detection Limits In EDXRF the detection limits are sample specific. They are influenced by matrix effects, line overlaps as well as signal processing of the detector. multiplied by a factor of 2.2. The detection limits of Mg, Al,, P and S have to be multiplied by 1.4 to estimate the detection limits at a measuring time of 10 seconds. In consideration of line overlaps, pile ups and other detector artifacts the Eval-Server calculates detection limits and displays them as analysis result. The LOD is calculated as 3 times standard deviation (SD). Table 1: Iron base Element LOD Al 0.4 Cd 0.02 Co 0.09 Cr 0.01 Cu 0.01 Mn 0.02 Mo 0.007 Nb 0.007 P 0.03 Pb 0.02 S 0.01 Sb 0.02 0.08 Sn 0.03 Ti 0.02 V 0.01 W 0.03 Zn 0.007 Zr 0.005 The following data are related to measurements of pure single element standards at a measuring time of 10 seconds for elements Z 21 respectively 20 seconds for Mg, Al,, P and S using a 4 µm polypropylene film between sample and measuring head. To estimate the detection limits at a measuring time of 2 seconds (instead of 10 seconds) the given values have to be Page 3/10
Table 2: Nickel base Element LOD Ag 0.03 Al 0.3 Cd 0.03 Co 0.01 Cu 0.06 Cr 0.02 Fe 0.01 Hf 0.05 Mn 0.01 Mo 0.01 Nb 0.01 Pb 0.04 Re 0.06 Sb 0.04 0.07 Sn 0.04 Ta 0.06 Ti 0.01 V 0.01 W 0.04 Zn 0.04 Table 3: Titanium base Element LOD Al 0.4 Cd 0.02 Co 0.02 Cr 0.01 Cu 0.007 Fe 0.006 Mn 0.009 Mo 0.007 Nb 0.003 Ni 0.009 Pd 0.02 Ru 0.01 0.08 Sn 0.02 Ta 0.07 V 0.1 Zn 0.005 Zr 0.004 Table 4: Cobalt base Element LOD Cd 0.03 Cr 0.01 Cu 0.01 Fe 0.02 Mn 0.01 Mo 0.007 Nb 0.007 Ni 0.07 Pb 0.03 0.07 Sn 0.04 Ta 0.07 Ti 0.01 V 0.01 W 0.04 Zn 0.009 Zr 0.009 Table 5: Copper base Element LOD Ag 0.03 Al 0.3 As 0.01 Au 0.04 Bi 0.03 Cd 0.03 Co 0.007 Fe 0.01 Mn 0.008 Ni 0.01 P 0.02 Pb 0.04 Sb 0.06 Se 0.009 0.07 Sn 0.05 Te 0.04 Ti 0.01 V 0.01 Zn 0.08 Page 4/10
Table 6: Aluminum base Element LOD Ag 0.003 Bi 0.003 Cd 0.004 Co 0.003 Cr 0.004 Cu 0.002 Fe 0.005 Mg 0.4 Mn 0.002 Mo 0.001 Nb 0.001 Ni 0.008 Pb 0.003 Sb 0.005 Sc 0.01 0.05 Sn 0.003 Ti 0.01 V 0.006 Zn 0.01 Zr 0.001 Table 7: Magnesium base Element LOD Ag 0.003 Al 0.2 Cd 0.003 Ce 0.02 Co 0.01 Cr 0.002 Cu 0.007 Fe 0.004 La 0.02 Mn 0.002 Mo 0.0008 Nb 0.001 Nd 0.04 Ni 0.008 Pb 0.009 Sb 0.004 0.01 Sn 0.004 Th 0.003 Ti 0.008 Y 0.003 Zn 0.009 Zr 0.001 Table 8: Lead base Element LOD Ag 0.1 As 0.1 Bi 0.2 Cd 0.02 Co 0.03 Cu 0.02 Fe 0.03 Cr 0.03 Mn 0.04 Ni 0.03 Pd 0.1 Sb 0.04 Sn 0.3 Ti 0.05 V 0.04 Zn 0.02 Page 5/10
Table 9: Tin base Element LOD Ag 0.08 Al 0.1 Cd 0.03 Co 0.01 Cr 0.01 Cu 0.008 Fe 0.01 Ge 0.01 Mn 0.01 Mo 0.004 Nb 0.004 Pb 0.02 Pd 0.02 Sb 0.06 0.1 Ti 0.06 V 0.02 Zn 0.008 Table 10: Zinc base Element LOD Ag 0.04 Al 0.4 Au 0.04 Bi 0.04 Cd 0.04 Co 0.01 Cr 0.01 Cu 0.02 Fe 0.008 Mn 0.01 P 0.04 Pb 0.04 Sb 0.05 Se 0.01 0.08 Sn 0.05 Ti 0.02 V 0.02 Table 11: Zirconium base Element LOD Ag 0.08 Al 0.4 Cd 0.07 Co 0.02 Cu 0.02 Cr 0.02 Fe 0.03 Hf 0.03 Mn 0.02 Mo 0.1 Nb 0.03 Pb 0.03 Sb 0.08 0.1 Sn 0.08 Ta 0.03 Ti 0.04 V 0.04 W 0.03 Zn 0.008 Table 12: Gold base Element LOD Ag 0.04 Co 0.02 Cu 0.02 Cr 0.04 Fe 0.03 Mn 0.02 Pd 0.2 Pt 0.2 Rh 0.05 Ru 0.05 Ti 0.05 V 0.04 Zn 0.05 Page 6/10
Table 13: Platinum base Element LOD Ag 0.03 Au 0.3 Co 0.01 Cu 0.02 Cr 0.03 Fe 0.02 Mn 0.03 Pd 0.04 Rh 0.05 Ru 0.05 Ti 0.04 V 0.05 W 0.6 Zn 0.01 6. Some Typical Measurement Examples pauses are used to correct possible gain shifts. This procedure guarantees reproducible and accurate results as shown in the tables at different and changing ambient temperatures. (: Analytical Standard Deviation) All data in mass percentage Table 14: Aluminum base 3003 AL Al 10s 97.18 97.77 Cu 5s 0.084 0.002 0.085 Fe 5s 0.632 0.006 0.64 Mn 5s 1.06 0.01 1.10 10s 0.31 0.04 30s 0.32 0.02 0.25 Zn 5s 0.019 0.001 0.020 4145 AB Al 10s 84.80 84.24 Cr 5s 0.038 0.003 0.050 Cu 5s 4.00 0.01 4.12 Fe 5s 0.526 0.005 0.54 Mg 10s <0.7 30s <0.5 0.050 Mn 5s 0.042 0.002 0.050 10s 10.20 0.11 30s 10.26 0.06 10.66 Zn 5s 0.051 0.002 0.058 5083 AF Al 10s 93.62 93.49 Cr 5s 0.156 0.004 0.15 Cu 5s 0.071 0.002 0.078 Fe 5s 0.341 0.005 0.34 Mg 10s 4.8 0.3 30s 5.0 0.2 4.85 Mn 5s 0.710 0.007 0.74 10s 0.16 0.03 30s 0.20 0.02 0.17 Ti 5s 0.031 0.003 0.027 Zn 5s 0.051 0.001 0.050 6061 SS Al 10s 96.84 97.81 Cr 5s 0.249 0.005 0.229 Cu 5s 0.308 0.003 0.30 Fe 5s 0.348 0.004 0.35 Mg 10s 1.4 0.3 30s 1.1 0.2 1.00 Mn 5s 0.047 0.003 0.052 10s 0.63 0.04 30s 0.65 0.02 0.64 Ti 5s 0.042 0.003 0.037 Zn 5s 0.081 0.002 0.080 Page 7/10
Table 15: Stainless and heat resisting steel AISI 303 Mn 2s 1.86 0.07 1.87 P S 10s 0.06 0.03 30s 0.07 0.02 10s 0.38 0.02 30s 0.33 0.01 10s 0.70 0.08 30s 0.55 0.05 0.032 0.378 0.634 Cr 2s 17.5 0.1 17.35 Ni 2s 8.97 0.11 8.64 Mo 2s 0.57 0.02 0.58 AISI 416 Mn 2s 0.37 0.06 0.35 P S 10s <0.05 30s 0.03 0.01 10s 0.29 0.02 30s 0.32 0.01 10s 0.39 0.07 30s 0.41 0.04 0.026 0.29 0.37 Cr 2s 12.22 0.08 12.25 Table 16: Aerospace materials 17-7PH Mn 2s 0,.62 0.07 0.76 P S 10s 0.05 0.02 30s <0.03 10s <0.04 30s <0.02 10s 0.43 0.07 30s 0.27 0.04 0.023 0.0019 0.361 Cr 2s 17.2 0.1 16.94 Ni 2s 7.4 0.1 7.22 Al 10s 1.3 0.3 30s 1.0 0.2 1.19 Table 17: Materials with special physical properties Nitronic 60 Mn 2s 8.7 0.1 8.58 10s 3.53 0.13 30s 3.88 0.08 3.67 Cr 2s 16.3 0.1 16.37 Ni 2s 8.6 0.1 8.5 Fe 2s 61.7 0.2 61.71 Table 18: 11% Manganese steel SS-CRM No. 493/1 Mn 2s 11.4 0.1 11.24 P 10s <0.061 30s 0.11 0.02 0.095 S 10s <0.05 30s 0.04 0.02 0.022 10s 0.81 0.09 30s 0.83 0.05 0.86 Cr 2s 0.12 0.02 0.14 Ni 2s 2.92 0.08 2.97 Mo 2s 0.90 0.02 0.94 Table 19: Copper base CDA 623 Al 10s 9.37 0.58 30s 9.84 0.35 9.19 Mn 2s 0.166 0.015 0.16 Fe 2s 2.10 0.04 2.13 Ni 2s 0.07 0.02 0.075 Cu 2s 87.8 88.4 CDA 706 Mn 2s 0.596 0.023 0.62 Fe 2s 1.35 0.040 1.30 Co 2s <0.029 0.013 Ni 2s 10.16 0.09 10.03 Cu 2s 87.6 87.9 Zn 2s 0.15 0.05 0.082 Page 8/10
Table 20: Nickel base Monel R405 10s 0.089 0.041 0.046 30s 0.067 0.022 Mn 2s 1.03 0.03 1.03 Fe 2s 1.26 0.03 1.31 Co 2s <0.042 0.02 Ni 2s 65.2 64.8 Cu 2s 32.3 0.2 32.3 RENE 142 Al 10s 5.18 0.47 6.13 30s 5.81 0.28 Cr 2s 6.58 0.080 6.98 Co 2s 12.02 0.10 11.81 Ni 2s 58.9 57.61 Mo 2s 1.53 0.03 1.51 Hf 2s 1.22 0.11 1.34 Ta 2s 6.01 0.18 6.3 W 2s 5.03 0.19 4.92 Re 2s 2.46 0.16 2.6 Table 21: Cobalt base Table 22: Titanium base Ti 6-6-2 Al 10s 4.70 0.38 5.57 30s 5.20 0.21 Ti 2s 85.7 85.5 V 2s 5.74 0.12 5.57 Fe 2s 0.55 0.02 0.56 Ni 2s 0.02 0.01 0.015 Cu 2s 0.53 0.02 0.51 Mo 2s 0.008 0.004 0.008 Sn 2s 2.23 0.05 1.99 Table 23: Magnesium base Mg 468 HL Mg 10s 95.24 96.14 30s 95.48 Mn 2s 0.26 0,01 0.2 Cu 2s 0.105 0,003 0.09 Zn 2s 2.63 0,01 2.52 La 2s 0.22 0,03 0.23 Ce 2s 0.59 0,04 0.6 Ultimet 1233 Cr 2s 25.4 0.20 25.4 Mn 2s 0.780 0.061 0.79 Fe 2s 3.30 0.070 2.99 Co 2s 53.8 53.4 Ni 2s 9.57 0.10 9.47 Nb 2s 0.020 0.010 0.016 Mo 2s 4.80 0.05 4.72 W 2s 2.34 0.10 2.39 Page 9/10
7. Conclusion With the SPECTRO it is possible to conduct laboratory-like analyses in a single measuring cycle that lasts only 2 seconds. For integration of the light elements Mg, Al,, P and S within a complete analysis or for sorting various aluminum and magnesium alloys only 10 additional seconds are necessary. During this process even the light elements are measured in air without complicated techniques like helium flushing or vacuum, simplifying operation decidedly. The Eval-Server corrects line-overlaps and all detector artifacts and determines the sample composition using fundamental parameter. The LODs listed in this report show excellent sensitivity of the SPECTRO. The typical analysis results demonstrate outstanding precision and accuracy. www.spectro.com GERMANY SPECTRO Analytical Instruments GmbH Boschstrasse 10 D-47533 Kleve Tel.: +49.2821.892 2102 Fax: +49.2821.892 2202 spectro.info@ametek.com U.S.A. SPECTRO Analytical Instruments Inc. 91 McKee Drive Mahwah, NJ 07430 Tel.: +1.800.548 5809 +1.201.642 3000 Fax: +1.201.642 3091 spectro-usa.info@ametek.com HONG KONG (Asia-Pacific) SPECTRO Analytical Instruments (Asia-Pacific) Ltd. Unit 1603, 16/F., Tower III Enterprise Square No. 9 Sheung Yuet Road Kowloon Bay, Kowloon Hong Kong Tel.: +852.2976 9162 Fax: +852.2976 9542 spectro-ap.sales@ametek.com Subsidiaries: CHINA: Tel +86.10.8526.2111, Fax + 86.10.8526.2141, spectro-china.info@ametek.com.cn, FRANCE: Tel +33.1.30 68 89 70, Fax +33.1.30 68 89 79, spectro-france.info@ametek.com, GREAT BRITAIN: Tel +44.1162.462950, Fax +44.1162.740160, spectro-uk.info@ametek.com, INDIA: Tel +91.22.61 96 82 00, Fax +91.22.28 36 36 13, sales.spectroindia@ametek.com ITALY: Tel: +39.02.94693.1, Fax +39.02.94693650, spectro-italy.info@ametek.com, JAPAN: Tel: +81.3.6809.2405, Fax: +81.3.6809.2410, spectro-japan.info@ametek.com, SWEDEN: Tel: +46.8.519-060 31, Fax: +46.8.519.060 34, spectro-nordic.info@ametek.com, SOUTH AFRICA: Tel +27.11.9794241, Fax +27.11.9793564, spectro-za.info@ametek.com. SPECTRO operates worldwide and is present in more than 50 countries. Please contact our headquarters for your local representative. SPECTRO 2011, Subject to modifications J-11, Rev. 0, Photos: SPECTRO. Page 10/10